CN111957979B - Auxiliary alloy powder for permanent magnet material, preparation method of auxiliary alloy powder and permanent magnet material - Google Patents
Auxiliary alloy powder for permanent magnet material, preparation method of auxiliary alloy powder and permanent magnet material Download PDFInfo
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- CN111957979B CN111957979B CN202010664215.9A CN202010664215A CN111957979B CN 111957979 B CN111957979 B CN 111957979B CN 202010664215 A CN202010664215 A CN 202010664215A CN 111957979 B CN111957979 B CN 111957979B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/023—Hydrogen absorption
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/002—Ferrous alloys, e.g. steel alloys containing In, Mg, or other elements not provided for in one single group C22C38/001 - C22C38/60
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/005—Ferrous alloys, e.g. steel alloys containing rare earths, i.e. Sc, Y, Lanthanides
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/10—Ferrous alloys, e.g. steel alloys containing cobalt
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
- H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
- H01F1/047—Alloys characterised by their composition
- H01F1/053—Alloys characterised by their composition containing rare earth metals
- H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
- H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
- H01F1/0571—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes
- H01F1/0575—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together
- H01F1/0577—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together sintered
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/041—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by mechanical alloying, e.g. blending, milling
Abstract
The invention relates to auxiliary alloy powder used by rare earth materials and a preparation method thereof, wherein the preparation method uses hydrogen-absorbing alloy as alloy raw material to carry out smelting to obtain an auxiliary alloy intermediate; smelting the alloy raw material to obtain an auxiliary alloy intermediate; hydrogen crushing the auxiliary alloy intermediate to obtain auxiliary alloy particles; and carrying out jet milling on the auxiliary alloy particles to obtain auxiliary alloy powder. The auxiliary alloy powder adopts alloy raw materials in a specific proportion, has better hydrogen absorption performance, can be crushed more quickly when hydrogen is crushed to obtain more uniform powder with smaller particle size, and thus the technical problem of introducing impurities due to overlong preparation flow is solved.
Description
[ technical field ] A method for producing a semiconductor device
The invention relates to the field of rare earth permanent magnet materials, in particular to a preparation method of auxiliary alloy powder for a rare earth permanent magnet material, the auxiliary alloy powder for the rare earth permanent magnet material prepared by the method, and the rare earth permanent magnet material prepared by the auxiliary alloy powder.
[ background of the invention ]
At present, the application of rare earth permanent magnet materials is increasingly wide, and meanwhile, new energy and environmental protection are increasingly concerned and become a trend of inevitable development, so that the requirement of high coercivity is provided for the used rare earth permanent magnet materials.
Rare earth permanent magnetic materials generally include a primary phase and a secondary phase, with the secondary phase generally being an alloy powder. In the prior art, materials of some special elements, such as transition metal elements of Co, cu, al, zr, nb and the like and rare earth elements of Pr, dy, tb, gd, ho and the like, are added in the preparation (smelting and metallurgy) process of the auxiliary phase. When the auxiliary phase is used for preparing the rare earth permanent magnet material, the elements can be partially or completely present in the main phase crystal grains, so that the auxiliary phase containing special elements and the main phase neodymium-iron-boron powder containing neodymium-iron-boron crystal grain units are mixed and sintered to prepare the rare earth permanent magnet material with excellent performance.
The existing preparation process of the auxiliary phase containing the special elements mainly comprises coarse crushing, ball milling, coarse crushing, screening and jet milling, the preparation process is long, impurities are easy to introduce in the preparation process, and the condition that fine alloy particles are in contact with oxygen exists in the preparation process, so that the final performance of the prepared rare earth permanent magnet material is seriously influenced, such as the coercive force of the rare earth permanent magnet material is reduced.
[ summary of the invention ]
In view of the above, there is a need to provide a new method for preparing an auxiliary alloy powder for permanent magnetic materials, so as to solve the above problems.
In addition, it is necessary to provide an auxiliary alloy powder prepared by the above preparation method of the auxiliary alloy powder.
In addition, a permanent magnet material prepared by applying the auxiliary alloy powder is also needed to be provided.
A preparation method of auxiliary alloy powder comprises the following steps:
step S1: preparing an alloy raw material, wherein the alloy raw material comprises a hydrogen absorption alloy, the hydrogen absorption alloy comprises a component R and a component A, and the atomic content ratio of the component R to the component A is 1; the component A is one or a mixture of Fe and Co in any ratio; the component R is a rare earth element;
step S2: smelting the alloy raw material to obtain an auxiliary alloy intermediate;
and step S3: hydrogen crushing the auxiliary alloy intermediate to obtain auxiliary alloy particles;
and step S4: and carrying out jet milling on the auxiliary alloy particles to obtain auxiliary alloy powder.
Preferably, in the step S2, the alloy raw material is smelted by ingot casting or strip casting.
Preferably, the step S3 includes:
s31: putting the auxiliary alloy intermediate into a hydrogen heat treatment furnace, starting a vacuum system, and vacuumizing until the air pressure in the furnace is a first air pressure;
and S32, filling hydrogen into the hydrogen heat treatment furnace to enable the air pressure in the furnace to reach a second air pressure and keeping the second air pressure until the auxiliary alloy intermediate absorbs hydrogen and is saturated, so that the auxiliary alloy intermediate absorbs the hydrogen and is crushed into auxiliary alloy particles.
Preferably, the first air pressure is not more than 5 × 10 -3 Pa。
Preferably, the second gas pressure is 0.1MPa.
Preferably, the alloy raw material further comprises a transition metal, and the transition metal is one or more of Cu, al, zr and Nb.
Preferably, in the alloy raw material, the mass percentage content of the transition metal is in the range of 0-10%.
An auxiliary alloy powder is prepared by the preparation method of the auxiliary alloy powder.
The permanent magnetic material is prepared by mixing the auxiliary alloy powder and the main phase alloy powder and sequentially carrying out sintering and tempering processes.
Preferably, the mass percentage of the auxiliary alloy powder in the permanent magnet material is less than or equal to 5%.
Preferably, the main phase alloy powder is neodymium iron boron powder.
The auxiliary alloy powder adopts alloy raw materials with a specific proportion, has better hydrogen absorption performance, can be more quickly crushed when hydrogen is crushed, and obtains more uniform powder with smaller particle size, thereby avoiding the technical problem of introducing impurities due to overlong preparation flow.
[ description of the drawings ]
FIG. 1 is a flow chart of the preparation of the secondary alloy powder according to the preferred embodiment of the present invention.
Fig. 2 is a flow chart of the preparation of the permanent magnetic material according to the preferred embodiment of the present invention.
The following detailed description will further illustrate the invention in conjunction with the above-described figures.
[ detailed description ] embodiments
In order to make those skilled in the art better understand the technical solution of the present invention, the following detailed description will be made with reference to the embodiments and the accompanying drawings.
Referring to fig. 1, a preferred embodiment of the present invention provides a method for preparing an auxiliary alloy powder, which includes the following steps:
step S1: preparing an alloy raw material, wherein the alloy raw material comprises a hydrogen absorption alloy, the hydrogen absorption alloy comprises a component R and a component A, and the atomic content ratio of the component R to the component A is (1); the component A is one or a mixture of Fe and Co in any ratio, wherein the component R is a rare earth element and comprises: lanthanum, cerium, praseodymium, neodymium, promethium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium, scandium, or yttrium. Specifically, the atomic content ratio of the component R to the component A is 1.
Step S2: smelting the alloy raw material by using a conventional ingot casting or strip casting process mode to obtain an auxiliary alloy intermediate, wherein the auxiliary alloy intermediate is an auxiliary alloy block or an auxiliary alloy sheet;
and step S3: and (3) carrying out hydrogen crushing on the auxiliary alloy intermediate to obtain auxiliary alloy particles. The method comprises the following specific steps: putting the auxiliary alloy intermediate into a hydrogen heat treatment furnace, starting a vacuum system to vacuumize until the air pressure in the furnace is a first air pressure, then filling hydrogen into the hydrogen heat treatment furnace to enable the air pressure in the furnace to reach a second air pressure and keeping the second air pressure for a period of time T, enabling the auxiliary alloy intermediate to absorb the hydrogen and to be crushed into auxiliary alloy particles, after the auxiliary alloy intermediate is saturated in hydrogen absorption, extracting residual hydrogen in the furnace, then filling inert gas into the furnace, taking out the auxiliary alloy particles, wherein the first air pressure is less than or equal to 5 x 10 -3 Pa, said second gas pressure being 0.1Mpa, and in at least one embodiment said time T is 1 hour;
and step S4: and (3) placing the auxiliary alloy particles into an air flow mill for air flow milling to obtain auxiliary alloy powder, wherein the particle size of the auxiliary alloy powder is less than or equal to 1.6 mu m.
In the step S1, the alloy raw material may further include a transition metal including, but not limited to, one or more of Cu, al, zr, and Nb, on the premise of not affecting the alloy phase formation of 1. In the alloy raw material, the mass percentage content of the transition metal is 0-10%.
The auxiliary alloy powder adopts alloy raw materials with a specific proportion, has better hydrogen absorption performance, can be more quickly crushed when hydrogen is crushed, and obtains more uniform powder with smaller particle size, thereby avoiding the technical problem of introducing impurities due to overlong preparation flow.
As shown in fig. 2, the present invention further provides a permanent magnetic material, which is prepared by mixing the above-mentioned auxiliary alloy powder and main phase alloy powder under the protection of inert gas to form a mixed powder; and (2) molding and orienting the mixed powder, and sequentially performing conventional sintering and tempering processes to obtain the sintered powder, wherein the sintering process is to sinter and compact the powder in a vacuum sintering furnace, and the tempering process needs to be performed for multiple times. In at least one embodiment, the auxiliary alloy powder and the main phase alloy powder are mixed under the protection of inert gas. The mass percentage content of the auxiliary alloy powder is less than or equal to 5 percent. The main phase alloy powder may be neodymium iron boron powder. In at least one embodiment, the Nd-Fe-B powder has a primary phase of Nd 2 Fe 14 B。
The present invention will now be described in detail with reference to specific examples, which are intended to be illustrative of preferred embodiments of the present invention and are not to be construed as limiting the invention thereto.
Example 1
Preparing alloy raw material Pr 1 Co 2 And smelting the alloy raw material by using a conventional ingot casting process to obtain an auxiliary alloy block.
Placing the auxiliary alloy blocks into a hydrogen heat treatment furnace, starting a vacuum system, and vacuumizing until the air pressure in the furnace is 5 multiplied by 10 -3 Pa, then filling hydrogen into the hydrogen heat treatment furnace to ensure that the pressure in the furnace reaches 0.1Mpa and is kept for 1 hour to obtain auxiliary alloy particles, pumping out the residual hydrogen in the furnace, then filling inert gas into the furnace, and taking out the auxiliary alloy particles.
And (3) putting the auxiliary alloy particles into an air flow mill for air flow milling to obtain auxiliary alloy powder with the particle size of 1.6 mu m for the permanent magnet material.
The auxiliary alloy powder for the rare earth permanent magnetic material has a chemical formula of Nd 2 Fe 14 And (3) mixing the neodymium iron boron powder of the B according to the mass ratio of 2.
Example 2
Provide Dy as an alloy raw material 1 Co 2 And smelting the alloy raw material by using a conventional ingot casting process to obtain an auxiliary alloy block.
Putting the auxiliary alloy block into a hydrogen heat treatment furnace, starting a vacuum system to vacuumize until the air pressure in the furnace is 5 multiplied by 10 -3 Pa, then filling hydrogen into the hydrogen heat treatment furnace to ensure that the pressure in the furnace reaches 0.1Mpa and keeps for 1 hour to obtain auxiliary alloy particles, pumping out the residual hydrogen in the furnace, then filling inert gas into the furnace, and taking out the auxiliary alloy particles.
And (3) placing the auxiliary alloy particles into an air flow mill for air flow milling to obtain auxiliary alloy powder with the particle size of 1.58 mu m for the permanent magnet material.
The auxiliary alloy powder for the rare earth permanent magnetic material has a chemical formula of Nd 2 Fe 14 And mixing the neodymium iron boron powder of B under the protection of inert gas according to the mass ratio of 2.
The neodymium iron boron powder used in examples 1 and 2 above and the permanent magnetic material obtained were tested for remanence, coercivity, magnetic energy product, squareness and density, the results of which are shown in table one.
Table one:
from the above table it can be seen that: the coercive force of the permanent magnetic material prepared from the auxiliary alloy powder and the main phase alloy powder in the embodiment 1 is improved by 1.58KOe under the conditions that heavy rare earth metal is not added and the remanence is hardly reduced. The rare earth permanent magnetic material prepared from the heavy rare earth-containing auxiliary alloy powder and the main phase alloy powder in example 2 has an obvious coercivity improvement effect, and the coercivity improvement range reaches 3.2KOe per 1% of dy.
The auxiliary alloy powder adopts alloy raw materials with a specific proportion, has better hydrogen absorption performance, can be more quickly crushed when hydrogen is crushed, and obtains more uniform powder with smaller particle size, thereby avoiding the technical problem of introducing impurities due to overlong preparation flow.
The process of crushing the auxiliary alloy powder in the vacuum furnace by using hydrogen is carried out in the environment without air and impurities, so that the obtained auxiliary phase alloy particles are not polluted by the air and the impurities and have higher purity and lower oxygen content, and the auxiliary alloy powder for the rare earth permanent magnet material obtained by jet milling has higher purity and lower oxygen content, so that the rare earth permanent magnet material prepared from the auxiliary alloy powder has higher coercive force. In addition, the preparation process of the auxiliary alloy powder for the rare earth permanent magnet material is simple and the cost is low.
It should be understood, however, that there is no intention to limit the invention to the specific embodiments described, but on the contrary, the intention is to cover all modifications, equivalents, and alternatives falling within the spirit and scope of the invention as defined by the appended claims.
Claims (11)
1. A preparation method of auxiliary alloy powder is characterized by comprising the following steps: the method comprises the following steps:
step S1: preparing an alloy raw material, wherein the alloy raw material comprises a hydrogen absorption alloy, the hydrogen absorption alloy comprises a component R and a component A, and the atomic content ratio of the component R to the component A is 1; the component A is one or a mixture of Fe and Co in any ratio; the component R is a rare earth element;
step S2: smelting the alloy raw material to obtain an auxiliary alloy intermediate;
and step S3: hydrogen crushing the auxiliary alloy intermediate to obtain auxiliary alloy particles;
and step S4: and carrying out jet milling on the auxiliary alloy particles to obtain auxiliary alloy powder.
2. The method for preparing an auxiliary alloy powder according to claim 1, characterized in that: in the step S2, the alloy raw material is smelted in a mode of ingot casting or strip casting.
3. The method for preparing an auxiliary alloy powder according to claim 1, characterized in that: the step S3 includes:
s31: putting the auxiliary alloy intermediate into a hydrogen heat treatment furnace, starting a vacuum system, and vacuumizing until the air pressure in the furnace is a first air pressure;
and S32, filling hydrogen into the hydrogen heat treatment furnace to ensure that the pressure in the furnace reaches a second pressure and keeping the second pressure until the auxiliary alloy intermediate absorbs hydrogen to be saturated, so that the auxiliary alloy intermediate absorbs the hydrogen and is crushed into auxiliary alloy particles.
4. A method of preparing the secondary alloy powder of claim 3, wherein: the first air pressure is less than or equal to 5 multiplied by 10 -3 Pa。
5. A method of preparing a secondary alloy powder according to claim 3, wherein: the second air pressure is 0.1Mpa.
6. The method of preparing the secondary alloy powder of claim 1, wherein: the alloy raw material also comprises transition metal, and the transition metal is one or more of Cu, al, zr and Nb.
7. The method of preparing the secondary alloy powder of claim 6, wherein: in the alloy raw material, the mass percentage content of the transition metal is 0-10%.
8. A secondary alloy powder, characterized by: the auxiliary alloy powder is prepared by the preparation method of the auxiliary alloy powder as claimed in any one of claims 1 to 7.
9. A permanent magnetic material is prepared by mixing auxiliary alloy powder and main phase alloy powder, then forming and orienting, and sequentially sintering and tempering, and is characterized in that: the auxiliary alloy powder is produced by the method for producing an auxiliary alloy powder according to any one of claims 1 to 7.
10. The permanent magnetic material of claim 9, wherein: the mass percentage of the auxiliary alloy powder in the permanent magnet material is less than or equal to 5 percent.
11. The permanent magnetic material of claim 9, wherein: the main phase alloy powder is neodymium iron boron powder.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103903824A (en) * | 2012-12-27 | 2014-07-02 | 比亚迪股份有限公司 | Rare earth permanent magnetic material and preparation method thereof |
| CN104752013A (en) * | 2013-12-27 | 2015-07-01 | 比亚迪股份有限公司 | Rare earth permanent magnetic material and preparation method thereof |
| CN107958760A (en) * | 2016-10-17 | 2018-04-24 | 中国科学院宁波材料技术与工程研究所 | A kind of rare earth permanent-magnetic material and preparation method thereof |
| CN109859920A (en) * | 2019-03-07 | 2019-06-07 | 南京理工大学 | A kind of highly resistance corrosion richness high abundance rare-earth permanent magnet and preparation method |
| CN110853856A (en) * | 2019-11-22 | 2020-02-28 | 安泰科技股份有限公司 | High-coercivity cerium-containing magnet and preparation method thereof |
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- 2020-07-10 CN CN202010664215.9A patent/CN111957979B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103903824A (en) * | 2012-12-27 | 2014-07-02 | 比亚迪股份有限公司 | Rare earth permanent magnetic material and preparation method thereof |
| CN104752013A (en) * | 2013-12-27 | 2015-07-01 | 比亚迪股份有限公司 | Rare earth permanent magnetic material and preparation method thereof |
| CN107958760A (en) * | 2016-10-17 | 2018-04-24 | 中国科学院宁波材料技术与工程研究所 | A kind of rare earth permanent-magnetic material and preparation method thereof |
| CN109859920A (en) * | 2019-03-07 | 2019-06-07 | 南京理工大学 | A kind of highly resistance corrosion richness high abundance rare-earth permanent magnet and preparation method |
| CN110853856A (en) * | 2019-11-22 | 2020-02-28 | 安泰科技股份有限公司 | High-coercivity cerium-containing magnet and preparation method thereof |
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